摘要
目的提升酸枣仁合剂质量控制水平。方法采用一测多评(QAMS)法同时检测制剂中13个指标性成分的含量,色谱柱为InertSustain C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.05%磷酸水溶液-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为258 nm(新芒果苷、芒果苷、异芒果苷),210 nm(斯皮诺素、6′′′-阿魏酰斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B、去氢茯苓酸、茯苓酸),280 nm(洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯),柱温为30℃,进样量为10μL。以斯皮诺素为内参物,计算其他12种待测成分的相对校正因子,测定含量并与外标法测定结果比较。建立灰色关联度和熵权优劣解距离(TOPSIS)模型对3个厂家12批样品质量进行综合评价。结果上述成分质量浓度依次在4.55~227.50μg/mL、2.46~123.00μg/mL、0.38~19.00μg/mL、1.79~89.50μg/mL、1.48~74.00μg/mL、1.35~67.50μg/mL、0.74~37.00μg/mL、0.46~23.00μg/mL、0.99~49.50μg/mL、0.62~31.00μg/mL、1.09~54.50μg/mL、2.15~107.50μg/mL、2.86~143.00μg/mL范围内与峰面积线性关系良好(r>0.9990);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为96.88%~100.12%,RSD为0.53%~1.55%(n=9)。上述12种待测成分的相对校正因子分别为0.7435,0.7981,4.1896,0.9173,1.1114,1.8832,2.9479,1.4835,2.1942,1.2689,0.8794,0.6918,12批样品13个待测成分采用外标法和QAMS法的含量测定结果无显著差异(P>0.05)。灰色关联度模型(分析法)所得相对关联度为0.3070~0.6141,熵权TOPSIS模型欧氏贴近度为0.2253~0.6306,2种模型对12批样品的综合质量评价结果基本一致,同一生产厂家样品质量相对稳定,不同生产厂家样品质量差异较大。结论所建立的QAMS法可用于酸枣仁合剂多组分定量检测;灰色关联度联合熵权TOPSIS模型可用于制剂质量的综合评价。
Objective To promote the quality control of Suanzaoren Mixture.Methods Quantitative analysis of multi-components by single marker(QAMS)method was used to simultaneously detect the content of 13 target ingredients in the preparation.The chromatographic column was InertSustain C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was 0.05%phosphoric acid aqueous solution-acetonitrile(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 258 nm(neomangiferin,mangiferin,isomangiferin),210 nm(spinosin,6′′′-feruloylspinosin,jujuboside A,jujuboside B,dehydropachymic acid,pachymic acid)and 280 nm(senkyunolide H,senkyunolide I,senkyunolide A,ligustilide),the column temperature was 30℃,and the injection volume was 10μL.The relative correction factors(RCFs)of the other 12 ingredients to be tested were calculated with spinosin as the internal reference,the content of ingredients were determined and compared with that by the external standard method(ESM).The grey relational analysis(GRA)and entropy weight-technique for order preference by similarity to ideal solution(EW-TOPSIS)model were established to comprehensively evaluate the quality of 12 batches of samples from three manufacturers.Results The linear ranges of the above 13 ingredients were 4.55-227.50μg/mL,2.46-123.00μg/mL,0.38-19.00μg/mL,1.79-89.50μg/mL,1.48-74.00μg/mL,1.35-67.50μg/mL,0.74-37.00μg/mL,0.46-23.00μg/mL,0.99-49.50μg/mL,0.62-31.00μg/mL,1.09-54.50μg/mL,2.15-107.50μg/mL,2.86-143.00μg/mL(r>0.9990)respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rate was in the range of 96.88%to 100.12%with RSDs of 0.53%to 1.55%(n=9).The RCFs of the above 12 ingredients to be tested were 0.7435,0.7981,4.1896,0.9173,1.1114,1.8832,2.9479,1.4835,2.1942,1.2689,0.8794,0.6918 respectively.The content of 13 ingredients in 12 batches of samples determined by the ESM and QAMS method was similar(P>0.05).The relative correlation degree in the GRA model was in the range of 0.3070 t
作者
王瑞芳
牟胜群
张秋红
WANG Ruifang;MU Shengqun;ZHANG Qiuhong(Jinan Maternity and Child Care Hospital Affiliated to Shandong First Medical University,Jinan,Shandong,China 250000;Jinan Food and Drug Inspection and Testing Center,Jinan,Shandong,China 271100)
出处
《中国药业》
CAS
2023年第24期90-98,共9页
China Pharmaceuticals
基金
山东省药学会科学技术项目[鲁药会[2020]18号]。
关键词
酸枣仁合剂
高效液相色谱法
一测多评法
相对校正因子
灰色关联度分析
熵权优劣解距离法
中成药
质量评价
Suanzaoren Mixture
HPLC
QAMS
relative correction factor
grey relational analysis
entropy weight-technique for order preference by similarity to ideal solution
Chinese patent medicine
quality evaluation
